CN102277491A - Novel process for extracting gallium from Bayer mother solution by using chelating resin - Google Patents
Novel process for extracting gallium from Bayer mother solution by using chelating resin Download PDFInfo
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Abstract
The invention discloses a novel process for extracting gallium from Bayer mother solution by using a chelating resin, which comprises the following steps: (1) fully washing, namely filling 6.5 to 2.5N of alkaline solution into a fully washing tower in a concentration gradient decrease manner to fully wash a saturated resin, and returning the effluent into an aluminum oxide plant; (2) rinsing, namely filling alkaline solution which has the same alkali concentration as an eluent into a rinsing tower for rinsing, filtering the effluent to remove suspended matters, recovering the effluent for preparing the eluent; and (3) performing transformation, namely filling 2.5 to 6N of alkaline solution into a transformation tower in a concentration gradient decrease manner to perform the transformation treatment of the resin, recovering part of the effluent to prepare eluent and recovering part of the effluent for use in transformation treatment in next period. When the novel process disclosed by the invention is used, the rises of the temperatures in the towers in the steps for extracting gallium by using chelating resin can be reduced obviously, the attenuation of the performance of the resin can be reduced, and the service life of the resin can be prolonged.
Description
Technical field
The present invention relates to a kind ofly from the Bayer mother liquor, extract the technology of gallium, belong to the hydrometallurgy field with resin.
Background technology
Gallium is a kind of dissipated metal, and important effect is arranged in semi-conductor industry, and the demand of gallium is also continuing to increase year after year.But, the source rareness of gallium, the many by products of its product from aluminium industry etc.Common containing metal gallium 0.002-0.008% in the bauxite.In the process of alumina producing Bayer process, the gallium in the bauxite has 70% approximately with aluminum oxide leaching together, and about 30% remains in the red mud.Along with the circulation of seed precipitation solution, the gallium concentration in the Bayer-process seed-separating mother liquor can be accumulated to 100-300ppm.
Technology with resin extraction gallium has become the main path that extracts gallium from the Bayer mother liquor at present.Existing technology with resin extraction gallium mainly may further comprise the steps:
(1) absorption: the Bayer mother liquor enters the adsorption tower that absorption gallium resin is housed by pump delivery, and gallium ion wherein is attracted on the resin, and the Bayer mother liquor after absorption turns back to alumina producer.Resin after the absorption delivers into the full tower of washing by air, and the resin of this moment is called saturated resin.
(2) full washing: water enters full washing in the tower by pump delivery, and the Bayer mother liquor that remains in the resin is rinsed well.Full wash liquid effluent and turn back to alumina producer.Resin after full the washing enters into the rinsing tower by pipeline, and the resin of this moment is called the resin after full the washing.
(3) rinsing: water enters in the rinsing tower by pump delivery, and remaining impurity in the resin of fragmentation and the resin is gone out, and the resin after the rinsing delivers in the eluting column by air, and the resin of this moment is called the resin after the rinsing.
(4) drip washing: eluent enters in the eluting column by pump delivery, and the gallium ion desorb that is adsorbed on the resin is got off to enter into solution.Eluent is about the Na of 73.5-107.2g/L by concentration
2S solution and alkali concn are that the mixed solution of the NaOH solution of 2.4-2.6N is formed.The drip washing effluent liquid is used for next step gallium extracting technology.Resin after drip washing delivers in tower transition by air, and the resin of this moment is called the poor resin after the drip washing.
(5) transition: water enters in tower transition by pump delivery, and the eluent that remains in the resin is rinsed well.Resin after transition delivers into the operational process that enters next cycle in the adsorption tower by air, and this moment, resin was called the poor resin after transition.
The working order of absorption gallium resin and stability except that with the distinctive physics of resin and chemical property mutually outside the Pass, ambient conditions especially temperature is to influence the working order of resin and the main factor of stability, temperature is too high can to produce fatefulue destruction to resin, causes the resin absorption capacity to descend significantly.Find that there is exothermic phenomenon in the alkaline solution of high density in dilution in the long-term production practice, the thermal discharge size is relevant with concentration difference, alkali lye system size and the system radiating situation of alkali lye dilution front and back.To wash operation be example with full: remaining in the saturated resin after the absorption have a large amount of mother liquors, alkali concn is 5-6N in the mother liquor, when water enters the full tower of washing resin is satisfied when washing, concentration difference is bigger between water and the remaining mother liquor, in the process that remaining mother liquor is replaced by water gradually, because the existence of the heat of dilution can produce a large amount of heat in a short time, cause that the full interior temperature of tower of washing raises rapidly, the loading capacity of resin obviously descends.The drip washing operation is to put forward the most serious operation section of heat release in the gallium production process.Through remaining big water gaging in the resin after the rinsing, when containing Na
2After the eluent of S and NaOH enters water remaining in eluting column and the resin and contacts, at S
2-Have very exothermic of following short period of time, turnover tower temperature contrast can be up to 30-40 ℃.Resin is inhaled the attenuation problem of gallium capacity, perplexs production for a long time always, investigates one by one through multi-faceted multi-angle, just finds the seriousness of heat of dilution problem.Rinsing, transition operation can have the replacement process of water and basic solution or basic solution and water equally, the concentration gradient variation all can cause the rapid rising of temperature short period of time, thereby causes the reduction of resin suction gallium capacity.
Summary of the invention
The present invention is according to existing Production Flow Chart and the resin properties that extracts gallium with resin, under absorption mother liquor and not change of eluent component situation, full wash, rinsing, transition use the alkaline solution of different gradients to substitute water in the present corresponding production process as medium in the operation, the concentration gradient that reduces alkali and water generates in the process changes, and eliminates temperature that the existence owing to the heat of dilution the produces phenomenon that sharply raises.
Specific embodiments of the present invention are as follows:
Treating processes of the present invention relate to resin fullly washing of extracting gallium, rinsing and transition operation.
The present invention adopt alkaline solution to absorption gallium resin satisfy wash, rinsing and transition manipulation.Concrete grammar is:
Use alkaline solution according to the concentration gradient mode of successively decreasing the full saturated resin of washing in the tower to be satisfied and wash processing, effluent liquid turns back to alumina producer.The alkali lye maximum concentration is 6N, and minimum concentration is 2.5N.The full soda liquid concentration gradient mode of successively decreasing is 6N-4N-2.5N, substitutes successively according to three concentration orders every 40min in the 2h; Be preferably 6N-5N-4N-3N-2.5N, substitute successively according to five concentration orders every 24min in the 2h; More preferably 6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N substitutes according to eight concentration orders successively every 15min in the 2h, and the resin after full the washing enters into the rinsing tower by pipeline.
Resin after using the alkaline solution identical with existing gallium extracting technology eluent alkali concn to full washing in the rinsing tower carries out rinsing to be handled, effluent liquid removes by filter and recyclablely behind the suspended substance is used to prepare eluent, and the resin after the rinsing delivers in the eluting column by air.
Use alkaline solution according to the processing that makes the transition of the poor resin of concentration gradient incremental manner after to drip washing in the transition tower, the alkali lye maximum concentration is 6N, and minimum concentration is 2.5N.Transition, concentration of lye gradient incremental manner was 2.5N-4N-6N, substituted successively according to three concentration orders every 40min in the 2h; Be preferably 2.5N-3N-4N-5N-6N, substitute successively according to five concentration orders every 24min in the 2h; More preferably 2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N substitutes according to eight concentration orders successively every 15min in the 2h.The effluent liquid part is recyclable to be used to prepare eluent, and part is handled the recyclable transition that is used for next cycle; Resin after transition delivers into the operational process that enters next cycle in the adsorption tower by air.
Adopt method of the present invention can obviously reduce degree with resin extracts that gallium is fullly washed, temperature raises in the tower in rinsing, drip washing, transition and the absorption process, full wash temperature and can descend 5-10 ℃, the rinsing temperature can descend 6-10 ℃, the drip washing temperature can descend 10-20 ℃, transition, temperature can descend 5-8 ℃, and adsorption temp can descend 2-5 ℃.Through simultaneous test contrast make that water and alkali are fullly being washed as medium, 5 all after date resin absorption performance datas are in rinsing, the transition operation: make water do medium, 5 all after date resin saturated adsorption capacities are 1.3-1.6g/L; Use alkaline solution to do medium, 5 all after date resin saturated adsorption capacities are 1.8-2.1 g/L; The latter exceeds 38% than the former resin absorption capacity.
Embodiment
Embodiment 1:
Under the same operational condition, respectively as medium, investigate temperature variations and resin absorption capacity in each operation process with water and sodium hydroxide solution.
With water as medium, temperature variations following (wherein inlet temperature of stabilizer, tower exit temperature round and detect data mean value in the process, and following examples are all identical) in each operation process:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 23 ℃, and going out the tower liquid temp is 34 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 23 ℃, and going out the tower liquid temp is 37 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent (proportioning pass away scape technology part), the leacheate inlet temperature of stabilizer is 20 ℃, tower exit temperature is 53 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 23 ℃, and going out the tower water temp is 35 ℃;
(5) absorption: the adsorption tower loaded resin is 20m
3, advancing mother liquid flow rate is 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 39 ℃, and going out tower mother liquor temperature is 46 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by air force feed tower.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times), get the resin after finishing, according to
GB/T-Gallium content is 1.5g/L 20975.20-2008 method detects wherein.
As medium, temperature variations is as follows in each operation process with sodium hydroxide solution:
(1) full washing: full to wash tower resin volume be 5m
3, 2m
3/ h, time 2h.Advancing tower alkali lye is sodium hydroxide solution, begin to be reduced to gradually 2.5N(6N-4N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts and generates a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 23 ℃, and going out the tower alkali liquid temperature is 28 ℃;
(2) rinsing: rinsing tower resin is volume 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, and concentration is 2.5N.Advancing the tower alkali liquid temperature is 23 ℃, and going out the tower alkali liquid temperature is 24 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent, alkali concn are 2.5N.The leacheate inlet temperature of stabilizer is 20 ℃, and tower exit temperature is 30 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, begin to increase to gradually 6N(2.5N-4N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 40min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 6N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 23 ℃, and going out the tower alkali liquid temperature is 29 ℃;
(5) absorption: the adsorption tower loaded resin is 20m
3, advancing mother liquid flow rate is 25m
3/ h, the treatment time is 2h.Advancing tower mother liquor temperature is 39 ℃, and going out tower mother liquor temperature is 42 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times), get the resin after finishing, according to
GB/T-Gallium content is 1.8 g/L 20975.20-2008 method detects wherein.
Be respectively medium with water and sodium hydroxide solution, the contrasting data of temperature variation and 5 all after date resin absorption amounts is as shown in table 1 in each operation process, the employing sodium hydroxide solution is a medium, can obviously improve the attenuation of each process temperature rising situation and resin absorption amount.
Table 1
Embodiment 2:
Under the same operational condition, respectively as medium, investigate each technological process temperature variations and resin absorption capacity with water and potassium hydroxide solution.
As medium, temperature variations is as follows in each operation process with water:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 35 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 23 ℃, and going out the tower liquid temp is 36 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 4m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent (proportioning pass away scape technology part), the leacheate inlet temperature of stabilizer is 22 ℃, tower exit temperature is 55 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 23 ℃, and going out the tower liquid temp is 32 ℃;
(5) absorption: the adsorption tower loaded resin is 20m
3, advancing mother liquid flow rate is 28m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 45 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by air force feed tower.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-20975.20-2008 it is 1.6 g/L that method detects its gallium content.
As medium, temperature variations is as follows in each operation process with potassium hydroxide solution:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, begin to be reduced to gradually 2.5N(6N-4N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N until the 2h end behind the 80min).Advancing the tower alkali liquid temperature is 22 ℃, and going out the tower alkali liquid temperature is 28 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, and concentration is 2.5N.Advancing the tower alkali liquid temperature is 22 ℃, and going out the tower alkali liquid temperature is 24 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 4m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent, leacheate inlet temperature of stabilizer are 21 ℃, and tower exit temperature is 29 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, begin to increase to gradually 6N(2.5N-4N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 40min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 6N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 22 ℃, and going out the tower alkali liquid temperature is 27 ℃;
(5) absorption: the adsorption tower loaded resin is 20m
3, advancing mother liquid flow rate is 28m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 42 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 1.8 g/L 20975.20-2008 method detects wherein.
Be respectively medium with water and potassium hydroxide solution, the contrasting data of temperature variation and 5 all after date resin absorption amounts is as shown in table 2 in each operation process, the employing potassium hydroxide solution is a medium, can obviously improve the attenuation of each process temperature rising situation and resin absorption amount.
Table 2
Embodiment 3:
Under the same operational condition, respectively as medium, investigate temperature variations and resin absorption capacity in each operation process with water and ammonia soln.
As medium, temperature variations is as follows in each operation process with water:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 33 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 38 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent (proportioning pass away scape technology part), the leacheate inlet temperature of stabilizer is 21 ℃, tower exit temperature is 54 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 22 ℃, and going out the tower liquid temp is 37 ℃;
(5) absorption: adsorption tower loaded resin 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 39 ℃, and going out tower mother liquor temperature is 43 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by air force feed tower.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 1.6 g/L 20975.20-2008 method detects wherein.
As medium, temperature variations is as follows in each operation process with ammonia soln:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, begin to be reduced to gradually 2.5N(6N-4N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 26 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, and concentration is 2.5N.Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 24 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2The S eluent.The leacheate inlet temperature of stabilizer is 21 ℃, and tower exit temperature is 30 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, begin to increase to gradually 6N(2.5N-4N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 40min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 6N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 21 ℃, and going out the tower alkali liquid temperature is 28 ℃;
(5) absorption: adsorption tower loaded resin 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 43 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 1.9 g/L 20975.20-2008 method detects wherein.
Be respectively medium with water and ammonia soln, the contrasting data of temperature variation and 5 all after date resin absorption amounts is as shown in table 3 in each operation process, and the employing ammonia soln is a medium, can obviously improve the attenuation of each process temperature rising situation and resin absorption amount.
Table 3
Embodiment 4:
Under the same operational condition, respectively as medium, investigate temperature variations and resin absorption capacity in each operation process with water and sodium hydroxide, potassium hydroxide, ammonia soln volume ratio 1:1:1 mixed solution (hereinafter to be referred as mixed alkali liquor).
As medium, each operation process temperature changing conditions is as follows with water:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 33 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 39 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2S eluent (proportioning pass away scape technology part), the leacheate inlet temperature of stabilizer is 19 ℃, tower exit temperature is 52 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower solution is water, and advancing the tower water temp is 21 ℃, and going out the tower liquid temp is 40 ℃;
(5) absorption: adsorption tower loaded resin 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 43 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by air force feed tower.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 1.6 g/L 20975.20-2008 method detects wherein.
As medium, temperature variations is as follows in each operation process with mixed alkali liquor solution:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is mixed alkali liquor, begin to be reduced to gradually 2.5N(6N-4N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 25 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, and concentration is 2.5N.Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 23 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2The S eluent.The leacheate inlet temperature of stabilizer is 19 ℃, and tower exit temperature is 31 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is mixed ammonium/alkali solutions, begin to increase to gradually 6N(2.5N-4N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 40min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 6N and finishes until 2h behind the 80min).Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 29 ℃;
(5) absorption: adsorption tower loaded resin 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 42 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 2.0 g/L 20975.20-2008 method detects wherein.
Table 4
Embodiment 5:
Under the same operational condition, as medium, investigate temperature variations and resin absorption capacity in each operation process with the sodium hydroxide solution of different concns gradient.
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, first group of concentration is that 6N-4N-2.5N(is designated as the A group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N and finishes until 2h behind the 80min).Second group of concentration is that 6N-5N-4N-3N-2.5N(is designated as the B group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 24min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 5N behind the 24min, the concentration of alkali is adjusted into 4N behind the 48min, and the rest may be inferred when 2h finishes, and the concentration of alkali is 2.5N).The 3rd group of concentration is that 6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N(is designated as the C group, and inflation method is with last same, pitch time 15min).It is average and go out tower medial temperature, data statistics such as table 5 to measure inlet temperature of stabilizer respectively:
Table 5
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, and concentration is 2.5N.
(3) transition: transition, tower resin volume was 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, and concentration is respectively 2.5N-4N-6N(and is designated as the A group), 2.5N-3N-4N-5N-6N(is designated as the B group), 2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N(is designated as the C group).Measure the tower medial temperature respectively and go out tower medial temperature, data statistics such as table 6:
Table 6
Embodiment 6
Under the same operational condition, as medium, investigate each process temperature changing conditions and resin absorption capacity with different concns gradient potassium hydroxide solution.
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, first group of concentration is that 6N-4N-2.5N(is designated as the A group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N and finishes until 2h behind the 80min).Second group of concentration is that 6N-5N-4N-3N-2.5N(is designated as the B group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 24min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 5N behind the 24min, the concentration of alkali is adjusted into 4N behind the 48min, and the rest may be inferred when 2h finishes, and the concentration of alkali is 2.5N).The 3rd group of concentration is that 6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N(is designated as the C group, and inflation method is with last same, pitch time 15min).Measure the tower medial temperature respectively and go out tower medial temperature, data statistics such as table 7:
Table 7
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, and concentration is 2.5N.
(3) transition: transition, tower resin volume was 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is potassium hydroxide solution, concentration is respectively 2.5N-4N-6N(and is designated as the A group), 2.5N-3N-4N-5N-6N(be designated as the B group), 2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N(is designated as the C group) measure the tower medial temperature respectively and go out tower medial temperature, data statistics such as table 8:
Table 8
Embodiment 7
Under the same operational condition, as medium, investigate each process temperature changing conditions and resin absorption capacity with different concns gradient ammonia soln.
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, first group of concentration is that 6N-4N-2.5N(is designated as the A group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 40min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 4N behind the 40min, and the concentration of alkali is adjusted into 2.5N until finishing behind the 80min).Second group of concentration is that 6N-5N-4N-3N-2.5N(is designated as the B group, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 24min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 5N behind the 24min, the concentration of alkali is adjusted into 4N behind the 48min, and the rest may be inferred when 2h finishes, and the concentration of alkali is 2.5N).The 3rd group of concentration is that 6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N(is designated as the C group, inflation method and last same).Measure inlet temperature of stabilizer and tower exit temperature respectively, data statistics such as table 9:
Table 9
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, and concentration is 2.5N.
(3) transition: transition, tower resin volume was 5m
3, flow velocity is 2.5m
3/ h, the treatment time is 2h.Advancing tower alkali lye is ammonia soln, concentration is respectively 2.5N-4N-6N(and is designated as the A group), 2.5N-3N-4N-5N-6N(be designated as the B group), 2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N(is designated as the C group) measure the tower medial temperature respectively and go out tower medial temperature, data statistics such as table 10:
Table 10
Embodiment 8 (running condition is investigated under the optimal conditions)
Under the same operational condition, as medium, investigate temperature variations and resin absorption capacity in each operation process with sodium hydroxide solution.
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, begin to be reduced to gradually 2.5N(6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 15min adjusts a concentration numerical value: the concentration of initial alkali is 6N, the concentration of alkali is adjusted into 5.5N behind the 15min, the concentration of alkali is adjusted into 5N behind the 30min, and the concentration of alkali is 2.5N when 2h finishes).Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 24 ℃;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is that concentration is the sodium hydroxide solution of 2.5N.Advancing tower alkali lye is 20 ℃ of temperature, and going out the tower alkali liquid temperature is 22 ℃;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h.Advancing tower solution is NaOH and Na
2The S eluent.The leacheate inlet temperature of stabilizer is 20 ℃, and tower exit temperature is 28 ℃;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h.Advancing tower alkali lye is sodium hydroxide solution, begin to increase to gradually 6N(2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 15min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, the concentration of alkali is adjusted into 3N behind the 15min, the concentration of alkali is adjusted into 3.5N behind the 30min, and the concentration of alkali is 6N when 2h finishes).Advancing the tower alkali liquid temperature is 20 ℃, and going out the tower alkali liquid temperature is 27 ℃;
(5) absorption: the adsorption tower loaded resin is 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h.Advancing tower mother liquor temperature is 40 ℃, and going out tower mother liquor temperature is 43 ℃.5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
More than (1)-(5) steps under the same operation condition, repeat 5 cycles (being circular flow 5 times).Get the resin after finishing, according to
GB/T-Gallium content is 2.1 g/L 20975.20-2008 method detects wherein.
Table 11
Above embodiment, or not within the spirit and principles in the present invention not all only for the purpose of description in order to restriction the present invention, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (12)
1. one kind is extracted the novel process of gallium with resin from the Bayer mother liquor, it is characterized in that comprising the steps:
(1) full washing: alkali lye according to the concentration gradient mode of successively decreasing enter full wash in the tower saturated resin satisfied wash, effluent liquid turns back to alumina producer;
(2) rinsing: concentration of lye is 2.4-2.6N in the current technology eluent, adopts the alkali lye identical with this eluent alkali concn to enter and carries out rinsing in the rinsing tower, and effluent liquid removes by filter and recyclablely behind the suspended substance is used to prepare eluent;
(3) transition: alkali lye enters in tower transition resin processings that make the transition according to the concentration gradient incremental manner, and the effluent liquid part is recyclable to be used to prepare eluent, recyclable processing transition that is used for next cycle of part.
2. according to the described novel process of claim 1, described alkali lye is the mixed solution of one or several solution in sodium hydroxide, potassium hydroxide, the ammonia soln.
3. according to the described novel process of claim 1, full soda liquid concentration is 6-2.5N.
4. according to claim 1, the full soda liquid concentration gradient mode of successively decreasing is 6N-4N-2.5N, substitutes successively according to three concentration orders every 40min in the 2h.
5. according to the described novel process of claim 1, the full soda liquid concentration gradient mode of successively decreasing is 6N-5N-4N-3N-2.5N, substitutes successively according to five concentration orders every 24min in the 2h.
6. according to the described novel process of claim 1, the full soda liquid concentration gradient mode of successively decreasing is 6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N, substitutes successively according to eight concentration orders every 15min in the 2h.
7. according to the described novel process of claim 1, the rinsing concentration of lye is identical with the eluent alkali concn.
8. according to the described novel process of claim 1, transition, concentration of lye was 2.5-6N.
9. according to the described novel process of claim 1, transition, concentration of lye gradient incremental manner was 2.5N-4N-6N, substituted successively according to three concentration orders every 40min in the 2h;
10. according to the described novel process of claim 1, transition, concentration of lye gradient incremental manner was 2.5N-3N-4N-5N-6N, substituted successively according to five concentration orders every 24min in the 2h.
11. according to the described novel process of claim 1, transition, concentration of lye gradient incremental manner was 2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N, substituted successively according to eight concentration orders every 15min in the 2h.
12. according to the described novel process of claim 1, a kind ofly from the Bayer mother liquor, extract the novel process of gallium, it is characterized in that may further comprise the steps with resin:
(1) full washing: full to wash tower resin volume be 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h; Advancing tower alkali lye is sodium hydroxide solution, begin to be reduced to gradually 2.5N(6N-5.5N-5N-4.5N-4N-3.5N-3N-2.5N according to the concentration gradient mode of successively decreasing from 6N, the alkali concn gradient is successively decreased and is regulated high alkali liquid and discharge proportioning by automatic control program, every interval 15min adjusts a concentration numerical value: the concentration of initial alkali is 6N, and the concentration of alkali is adjusted into 5.5N behind the 15min; The concentration of alkali is adjusted into 5N behind the 30min, and the concentration of alkali is 2.5N when 2h finishes;
(2) rinsing: rinsing tower resin volume is 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h; Advancing tower alkali lye is that concentration is the sodium hydroxide solution of 2.5N;
(3) drip washing: eluting column list tower resin volume is 5m
3, flow velocity is 5m
3/ h, the treatment time is 2h; Advancing tower solution is NaOH and Na
2The S eluent;
(4) transition: transition, tower resin volume was 5m
3, flow velocity is 2m
3/ h, the treatment time is 2h; Advancing tower alkali lye is sodium hydroxide solution, begin to increase to gradually 6N:2.5N-3N-3.5N-4N-4.5N-5N-5.5N-6N according to the concentration gradient incremental manner from 2.5N, the alkali concn gradient increases progressively by automatic control program regulates high alkali liquid and discharge proportioning, the about 15min in every interval adjusts a concentration numerical value: the concentration of initial alkali is 2.5N, and the concentration of alkali is adjusted into 3N behind the 15min; The concentration of alkali is adjusted into 3.5N behind the 30min, and the concentration of alkali is 6N when 2h finishes;
(5) absorption: the adsorption tower loaded resin is 20m
3, advance mother liquid flow rate 25m
3/ h, adsorption time are 2h; 5m after 2h finishes
3Resin enters into to satisfy by air force feed tower washes tower, will make the transition in addition and finish 5m afterwards
3Resin enters into adsorption tower by the air force feed.
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| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN109179467A (en) * | 2018-09-30 | 2019-01-11 | 中铝山东有限公司 | A method of gallium is removed to the low pregnant Bayer process liquor of concentration containing gallium |
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| CN101962713A (en) * | 2010-10-29 | 2011-02-02 | 西安蓝晓科技有限公司 | Continuous ion exchange device and method for extracting gallium from Bayer mother solution |
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| CN103382531A (en) * | 2012-05-04 | 2013-11-06 | 中国科学院过程工程研究所 | Method for enriching gallium from mother-liquor in technology for producing alumina from high-alumina fly ash |
| CN103382531B (en) * | 2012-05-04 | 2015-09-30 | 中国科学院过程工程研究所 | A kind of method of producing enrichment gallium alumina technology mother liquor from aluminous fly-ash |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN109179467A (en) * | 2018-09-30 | 2019-01-11 | 中铝山东有限公司 | A method of gallium is removed to the low pregnant Bayer process liquor of concentration containing gallium |
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